Abstract
In this study, a convenient and sensitive method for the determination of phthalate esters (PAEs) in plastic bottled water was proposed by on-line in-tube solid-phase microextraction (IT-SPME) coupled with high-performance liquid chromatography (HPLC). A hybrid monolithic column was synthesized with octamethacrylate substituted polyhedral oligomeric silsesquioxane (POSS-MA) as cross-linker and N-butyl methacrylate (BMA) as functional monomer, which was utilized as the extraction phase of IT-SPME. A number of important extraction parameters were systematically optimized, such as sampling flow rate, desorption solvent flow rate and volume, sample volume, and sample pH value. Under the optimal experimental conditions, the linear ranges of five PAEs were in the range of 0.1–60 ng mL−1. The limits of detection were between 0.052 and 0.10 ng mL−1, and the limits of quantification were less than 0.33 ng mL−1. In addition, the intra-day and inter-day relative standard deviations of the method were 0.98–3.0% and 2.0–4.3%, respectively. The EFs of the method for five PAEs were more than 538. The proposed method was also successfully applied to analyze trace PAEs in real samples with good recoveries. The recoveries of this method ranged from 84.6 to 111.6% and the relative standard deviations were less than 4.5%. The extraction recoveries of the prepared hybrid monolithic column of the target PAEs did not decrease significantly within 60 cycles. The results showed that the on-line IT-SPME-HPLC method was sensitive, highly efficient, and operationally convenient.
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This study was funded by the National Natural Science Foundation of China (No. 21677115), and Shaanxi Provincial Key Research and Development Program (No. 2019SF-238).
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Liulin Wei declares that he has no conflict of interest. Jie Liu declares that she has no conflict of interest. Qian Liu declares that she has no conflict of interest. **aomei Chen declares that she has no conflict of interest. Zhiqiang Li declares that she has no conflict of interest. Yidong Xu declares that she has no conflict of interest. Xueyun Gao declares that he has no conflict of interest. **aoxiao Lu declares that he has no conflict of interest. Zhian Guo declares that he has no conflict of interest. **gchan Zhao declares that he has no conflict of interest.
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Wei, L., Liu, J., Liu, Q. et al. Polyhedral Oligomeric Silsesquioxane–Based Hybrid Monolithic Column On-line In-Tube Solid-Phase Microextraction Coupled with High-Performance Liquid Chromatography for the Determination of Five Phthalate Esters in Bottled Water. Food Anal. Methods 15, 1107–1117 (2022). https://doi.org/10.1007/s12161-021-02180-4
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DOI: https://doi.org/10.1007/s12161-021-02180-4